Hydrochloric Acid → (4-(Trifluoromethyl)benzyl)malononitrile

HRID 749598

반응식

HRID 749598 반응식
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:14]=[CH:13][C:6]([CH:7]=[C:8]([C:11]#[N:12])[C:9]#[N:10])=[CH:5][CH:4]=1.[BH4-].[Na+].Cl>C(O)C>[F:1][C:2]([F:15])([F:16])[C:3]1[CH:4]=[CH:5][C:6]([CH2:7][CH:8]([C:11]#[N:12])[C:9]#[N:10])=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 714296(4-(Trifluoromethyl)benzylidene)malononitrileHCID 4311764Sodium borohydride

생성물 1

HCID 10656743(4-(Trifluoromethyl)benzyl)malononitrile수율 51.3%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

First, 4.44 g of (4-(trifluoromethyl)benzylidene)malononitrile was dissolved in 20 ml of ethanol, and while stirring at room temperature, a suspension of 0.19 g of sodium borohydride in 5 ml of ethanol was added dropwise, followed by stirring at room temperature for 30 minutes. Then, 10% hydrochloride acid was added to the reaction mixture, which became acidic and was extracted with diethyl ether. The organic layer was successively washed with 10% hydrochloric acid, a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 2.30 g of (4-(trifluoromethyl)benzyl)malononitrile (the intermediate (4)).

후처리

  1. additionwas added dropwise
  2. stirringby stirring at room temperature for 30 minutes
  3. extractionwas extracted with diethyl ether
  4. washThe organic layer was successively washed with 10% hydrochloric acid
  5. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d8439fc2695e4fb0b52aae099c3403eb
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402691B2

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